CN102502643B - Method for realizing resource recycling of silicon powder components in waste mortar from crystalline silicon cutting - Google Patents
Method for realizing resource recycling of silicon powder components in waste mortar from crystalline silicon cutting Download PDFInfo
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- CN102502643B CN102502643B CN2011102946029A CN201110294602A CN102502643B CN 102502643 B CN102502643 B CN 102502643B CN 2011102946029 A CN2011102946029 A CN 2011102946029A CN 201110294602 A CN201110294602 A CN 201110294602A CN 102502643 B CN102502643 B CN 102502643B
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Abstract
The invention discloses a method for realizing resource recycling of silicon powder components in waste mortar from crystalline silicon cutting. The method includes homogenate, cyclone separation, filter-press separation, aftertreatment (acid pickling, solvent washing and drying) of solid materials and the like. Homogenizing agent is adopted in process of the method, usage of dilute water is greatly reduced, and comprehensive purposes of homogenate, reduction of viscosity of a system and improved dispersion are achieved. The process of the method is based on matching of cyclone separation process and filter-press separation process, circulation supplementation of filter-press filter liquor is obtained by light-phase suspension, a separation effect of cyclone of fluid is sufficiently utilized, and accordingly, silicon powder components in heavy-phase mortar materials are continuously carried into the light-phase suspension so as to be recycled. Resource recycling rate of the silicon powder components in the waste mortar from crystalline silicon cutting can reach 88% at least.
Description
Technical field
The present invention relates to a kind of resource recycle method of crystalline silicon cutting waste mortar, particularly relate to a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silicon carbide component.Its Application Areas is mainly that the resource utilization of photovoltaic industry crystalline silicon cutting waste mortar, electron trade crystalline silicon cutting waste mortar reclaims and utilizes.Reclaim the silica flour component that obtains in the present invention and can obtain the HIGH-PURITY SILICON material through being further purified from waste mortar, have industrial application value widely.
Background technology
Silicon chip is the important foundation of development solar energy industry.Along with developing rapidly of solar energy industry in global range, silicon chip demand and amount of finish gather growth.According to the industry statistic data, Chinese silicon chip production capacity has been sure to occupy the whole world from 2008 the first, and the nearly 14GW of domestic silicon chip aggregated capacity in 2010 has accounted for global aggregated capacity more than 50%.
The line cutting is the current mode that present silicon chip is in the world produced.The process of line cutting processing depends on being used in conjunction with of crystal silicon cutting liquid (claim not only cutting fluid, suspension), silicon carbide micro-powder (but also claiming abrasive material, cutting sand), simultaneously can a large amount of crystalline silicon cutting waste mortar of association.According to the average state of the art of domestic silicon chip enterprise, the 1MW silicon chip approximately need consume 12 tons of crystalline silicons; 1 ton of crystalline silicon of every cutting approximately needs to use 3.0 tons of silicon carbide micro-powders and 3.2 tons of crystal silicon cutting liquids, and produces approximately 7.6～7.9 tons of cutting waste mortars in cutting process.According to the statistic data of domestic silicon chip industry in 2010, to expect 2012, domestic silicon chip enterprise's year needs approximately 115.2 ten thousand tons of silicon carbide micro-powders, approximately 122.88 ten thousand tons of crystal silicon cutting liquids, approximately 3,000,000 tons of year generation cutting waste mortar total amounts.
The main component of cutting waste mortar is cutting liquid component, silicon carbide, silica flour and metallic impurity.As everyone knows, have an appointment 50% crystal silicon of crystal silicon cutting cutting link is cut into silica flour and enters into waste mortar, effectively reclaims and comprehensive utilization technique owing to lacking, and annual t crystal silicon materials up to ten thousand are lost in vain.All by high energy consumption, expensive obtaining, its marketable value is much larger than auxiliary materials such as silicon carbide, cutting liquids for monocrystalline and polysilicon; If can be recycled for the discarded crystal silicon component of silicon chip production link, make it embody due recycling economy and be worth, have undoubtedly extremely huge economy, society and environmental benefit.
With regard to the cutting waste mortar, wherein comprise the recovery value of Si component far away higher than silicon carbide and cutting liquid.If can effectively reclaim the Si component in cutting slurry, develop corresponding comprehensive utilization technique, will produce huge commercial value.Therefore, research is reclaimed the silica flour component from the cutting waste mortar, realize the Si comprehensive utilization of resources, is not only the urgent need of Present Domestic theCourse of PV Industry, is also simultaneously the significant effort direction of environment protection, resource consumption reduction, has wherein contained huge business opportunities.
At present, reclaim both at home and abroad the industrial technology of high purity silica flour is that all right ripe from mortar, also there is no in the world corresponding industrialization precedent.2007, Xi'an Communications University has reported a kind of method that reclaims silica flour and carborundum powder from the cutting waste mortar in patent of invention 200710018636.9, it carries out solid-liquid separation to waste mortar, remove suspension agent and binding agent in waste material by organic solvent, solid-state sand material is carried out gas flotation, obtain the Si powder of certain purity, further this Si powder is carried out liquid floatation and gravitational segregation, again the silica flour that sub-elects is carried out pickling, obtain highly purified silica flour.The mixed powder of silicon carbide one metal that simultaneously gravitational segregation is obtained carries out magnetic separating, obtains pure silicon carbide powder.2008, the people such as T.Y Wang obtained HIGH-PURITY SILICON by the cutting slug is carried out the steps such as processing in early stage, acid treatment, pyroprocessing, directional freeze.2009, Y.F Wu, Y.M Chen research is carried out separation test by the effect of gravity and electric field, and the massfraction of the silicon carbide in slip is reduced to 7.15%.The recovery technology of external PV Silicon Forschungs und Produktions AG (Germany), SHARP KABUSHIKI KAISHA (Japan), Cobot Microelactronics Corp. (U.S.) silicon component in 2008 have reported some waste mortar systems later successively.At present, the distance of above-mentioned technology distance commercial application, formation industry size is also quite remote.
Summary of the invention
The object of the invention is to realize a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, in order to further obtain the HIGH-PURITY SILICON material by purifying.
The object of the present invention is achieved like this: a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, it is characterized in that the method comprises the following steps:
(1) homogenate: add leveler in crystalline silicon cutting waste mortar, every 100 parts of crystalline silicon cutting waste mortars by weight ratio, 2～20 parts of levelers, 30～500 parts, water; Described leveler is one or more in fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene; Control stirring velocity 50～200r/min; Homogenized temperature is room temperature or 50-80 ℃, 0.5～5.0 hour homogenate time;
(2) cyclonic separation: the mortar material by cyclone separator after with homogenate carries out cyclonic separation, and the feeding manner of mortar material adopts continuously or the intermittent feeding mode; The cyclonic separation temperature is room temperature or 50-80 ℃; Light phase suspension is constantly discharged by upper spillway, and the press filtration that is used for (3) after collecting separates; The heavy phase slurry is in the continuous enrichment of lower spillway, to the detection of taking a sample of the heavy phase slurry of the continuous enrichment of spillway under cyclone separator, when the weight percent of Si: SiC in the heavy phase slurry system reach 1: 15～1: 100 the time, constantly collect the heavy phase slurry by lower spillway, keep the weight percent of Si: SiC in collected gained heavy phase slurry between 1: 15～1: 100, gained heavy phase slurry B is used for reclaiming the silicon carbide component;
(3) press filtration separates: light phase suspension is carried out press filtration, obtain filtrate and filter residue; The press filtration separation temperature is room temperature or 50-80 ℃; Constantly collect filter residue, the solid-state material C of gained press filtration is used for reclaiming the silica flour component; In gained filtrate, 10～50% (v/v) circulation adds to described in (2) in cyclone separator, constantly collects all the other 50～90% filtrates (v/v), and gained press filtration filtrate A is used for reclaiming the cutting component;
(4) solid-state material aftertreatment: the solid-state material C of press filtration is carried out pickling, solvent wash, after gained silica flour wet feed drying, obtain the silica flour component.
Of the present invention a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, it is characterized in that: crystalline silicon cutting waste mortar comprises the crystalline silicon cutting waste mortar of photovoltaic industry and the crystalline silicon cutting waste mortar of electron trade.
Of the present invention a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, it is characterized in that: the acid used of pickling described in step (4) is mineral acid or organic acid, perhaps the mixture of organic acid and mineral acid; Described acid is pure acid or acid solution, and temperature is normal temperature or at 50 ℃～120 ℃; Comprise acetone, butanone, methyl alcohol, ethanol, Virahol, vinyl acetic monomer, sherwood oil, benzene, toluene, methylene dichloride, chloroform, ethylene dichloride, trieline, tetrahydrofuran (THF), second eyeball, propylene glycol, ethylene glycol, ethylene glycol monomethyl ether, glycol dimethyl ether, 1 with solvent during solvent wash, the mixture of one or more in the 4-dioxane, wash temperature is normal temperature or at 50 ℃～120 ℃, obtains the silica flour wet feed through mechanical separation again after cleaning.
Of the present invention a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silicon carbide component, its characteristic is: described in step (4) when oven dry silica flour wet feed furnace drying method used comprise fluid-bed drying, fixed bed drying method; 60 ℃～130 ℃ of bake out temperatures; Oven dry pressure comprises normal pressure or vacuum.
The present invention compared with prior art, its advantage is:
(1) technique of the present invention is by the use of leveler, decrease the consumption of dilution water, when reaching the purposes such as homogenate and reduction system viscosity, make the high molecular polymer in the waste mortar system be unwind, make the aggregate in the waste mortar system be dispersed.
(2) technique of the present invention is based on the realization of cyclonic separation technique, can be so that in the waste mortar system, the overwhelming majority in the silica flour component enters into light phase suspension, and then obtain being rich in the solid-state material of press filtration of Si component by the means that press filtration separates, to be used for reclaiming silica flour.
(3) technique of the present invention is based on the cooperation of cyclonic separation and press filtration separating technology, circulation by light phase suspension gained press filtration filtrate replenishes, take full advantage of the separating effect of fluid eddy flow, Si component in the heavy phase slurry constantly is entrained in light phase suspension goes, in order to recycle; Simultaneously, due to the reduction of Si component content in the heavy phase slurry, also greatly reduce the wastewater discharge of the recovery of silicon carbide component and purification link, reduce the pollutent generation; On the other hand, the cooperation of cyclonic separation and press filtration separating technology and the circulation of press filtration filtrate replenish the job state of also being convenient to reach quite stable in the process of production operation, are convenient to the raising of serialization production and production efficiency.
(4) technique of the present invention leveler used is one or more in fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene, it is exactly often the necessary component of crystal silicon cutting liquid product, and above-mentioned leveler can not bring disadvantageous effect to recovery, preparation and the cycle applications of cutting processing component after entering into press filtration filtrate.
(5) in the crystalline silicon cutting waste mortar of technique of the present invention, the resource utilization rate of recovery of silica flour component can reach more than 88%.
Description of drawings
Accompanying drawing is process flow sheet of the present invention.
Embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment 1:
Get a collection of crystalline silicon cutting waste mortar that LDK solar LDK sun power high-tech share company limited produces that derives from, waste mortar component principle condition is as follows after testing: cutting liquid component 42.0%, silicon carbide component 39.0%, silicon component 10.0%, moisture content 5.0%, metal species component 1.8%, pigment and cross-linked polymer material 2.2%.
10 tons of above-mentioned crystalline silicon cutting waste mortars are poured in steel basin, add 500Kg peregal O-25,10 tons of water; Open and stir and heat riser, mixing speed 80r/min is warmed up to 60 ℃ and insulation; Homogenate churning time 2 hours.Be transported in FXJ-50 type cyclone separator through the mode of the mortar material after homogenate with continuously feeding above-mentioned, keeping the cyclonic separation temperature is 60 ℃ and insulation, starts cyclone separator after 15 minutes, and beginning is collected light phase suspension at upper spillway.By transferpump, above-mentioned light phase suspension is transported to pressure filter and carries out press filtration, keep 55 ℃ of press filtration separation temperatures, constantly collect the press filtration filter residue standby in the solid-state material receiving tank of press filtration.
When collecting the press filtration filter residue, 25% (v/v) circulation in gained filtrate is added in above-mentioned FXJ-50 type cyclone separator, control the input speed of mortar material and the additional speed of press filtration filtrate, to guarantee that operating load is no more than the design objective of FXJ-50 type cyclone separator, constantly collect the press filtration filtrate (being used for reclaiming the cutting liquid component) of all the other 75% (v/v).
After FXJ-50 type cyclone separator moves 20 minutes, the sampling of spillway counterweight phase mortar detects under cyclone separator, Si in the heavy phase slurry system: the SiC weight percent is 1: 40, and constantly collect heavy phase slurry (be used for reclaim silicon carbide component) by lower spillway this moment.
The solid-state material of press filtration in the solid-state material receiving tank of press filtration is transported to 20% hydrochloric acid after stirring 1.5h under 50 ℃, enter separating centrifuge, after removing most of liquid, use again acetone after stirring 2h under 50 ℃, enter separating centrifuge, after removing most of liquid, adopt the dry 3h of fluidized-bed normal pressure under 80 ℃, collect the powder material 883Kg through super-dry, be the silica flour component.
Calculate and get, in the present embodiment, the resource utilization rate of recovery of silica flour component approximately 88.30%.
Embodiment 2:
Get a collection of crystalline silicon cutting waste mortar that prosperous photovoltaic Science and Technology Ltd. of Suzhou association produces that derives from, waste mortar component principle condition is as follows after testing: cutting liquid component 40.7%, silicon carbide component 38.4%, silicon component 11.3%, moisture content 5.5%, metal species component 1.9%, pigment and cross-linked polymer material 2.2%.
20 tons of above-mentioned crystalline silicon cutting waste mortars are poured in steel basin, add 900Kg emulsifier op-10,15 tons of water; Open and stir and heat riser, mixing speed 70r/min is warmed up to 55 ℃ and insulation; Homogenate churning time 2.5 hours.Be transported in FXJ-75 type cyclone separator through the mode of the mortar material after homogenate with continuously feeding above-mentioned, keeping the cyclonic separation temperature is 55 ℃ and insulation, starts cyclone separator after 25 minutes, and beginning is collected light phase suspension at upper spillway.By transferpump, above-mentioned light phase suspension is transported to pressure filter and carries out press filtration, keep 55 ℃ of press filtration separation temperatures, constantly collect the press filtration filter residue standby in the solid-state material receiving tank of press filtration.
When collecting the press filtration filter residue, 30% (v/v) circulation in gained filtrate is added in above-mentioned FXJ-75 type cyclone separator, control the input speed of mortar material and the additional speed of press filtration filtrate, to guarantee that operating load is no more than the design objective of FXJ-75 type cyclone separator, constantly collect the press filtration filtrate (being used for reclaiming the cutting liquid component) of all the other 75% (v/v).
After FXJ-75 type cyclone separator moves 35 minutes, the sampling of spillway counterweight phase mortar detects under cyclone separator, Si in the heavy phase slurry system: the SiC weight percent is 1: 35, and constantly collect heavy phase slurry (be used for reclaim silicon carbide component) by lower spillway this moment
The solid-state material of press filtration in the solid-state material receiving tank of press filtration is transported to 30% sulfuric acid after stirring 2h under 50 ℃, enter separating centrifuge, after removing most of liquid, use again acetoneand ethyl acetate mixed solvent (volume ratio 1: 3) after stirring 1.5h under 60 ℃, enter separating centrifuge, after removing most of liquid, adopt fixed bed vacuum-drying 3h under 80 ℃, collect the powder material 1997Kg through super-dry, be the silica flour component.
Calculate and get, in the present embodiment, the resource utilization rate of recovery of silica flour component approximately 88.36%.
Claims (4)
- One kind from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, it is characterized in that the method comprises the following steps:(1) homogenate: add leveler in crystalline silicon cutting waste mortar, every 100 parts of crystalline silicon cutting waste mortars by weight ratio, 2～20 parts of levelers, 30～500 parts, water; Described leveler is one or more in fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene; Control stirring velocity 50～200r/min; Homogenized temperature is room temperature or 50-80 ℃, 0.5～5.0 hour homogenate time;(2) cyclonic separation: the mortar material by cyclone separator after with homogenate carries out cyclonic separation, and the feeding manner of mortar material adopts continuously or the intermittent feeding mode; The cyclonic separation temperature is room temperature or 50-80 ℃; Light phase suspension is constantly discharged by upper spillway, and the press filtration that is used for (3) after collecting separates; The heavy phase slurry is in the continuous enrichment of lower spillway, to the detection of taking a sample of the heavy phase slurry of the continuous enrichment of spillway under cyclone separator, when the weight percent of Si: SiC in the heavy phase slurry system reach 1: 15～1: 100 the time, constantly collect the heavy phase slurry by lower spillway, keep the weight percent of Si: SiC in collected gained heavy phase slurry between 1: 15～1: 100, gained heavy phase slurry B is used for reclaiming the silicon carbide component;(3) press filtration separates: light phase suspension is carried out press filtration, obtain filtrate and filter residue; The press filtration separation temperature is room temperature or 50-80 ℃; Constantly collect filter residue, the solid-state material C of gained press filtration is used for reclaiming the silica flour component; In gained filtrate, 10～50% (v/v) circulation adds to described in (2) in cyclone separator, constantly collects all the other 50～90% filtrates (v/v), and gained press filtration filtrate A is used for reclaiming the cutting component;(4) solid-state material aftertreatment: the solid-state material C of press filtration is carried out pickling, solvent wash, after gained silica flour wet feed drying, obtain the silica flour component.
- According to claim 1 a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, it is characterized in that: crystalline silicon cutting waste mortar comprises the crystalline silicon cutting waste mortar of photovoltaic industry and the crystalline silicon cutting waste mortar of electron trade.
- According to claim 1 a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silica flour component, it is characterized in that: the acid used of pickling described in step (4) is mineral acid or organic acid, perhaps the mixture of organic acid and mineral acid; Described acid is pure acid or acid solution, and temperature is normal temperature or at 50 ℃～120 ℃; Comprise acetone, butanone, methyl alcohol, ethanol, Virahol, vinyl acetic monomer, sherwood oil, benzene, toluene, methylene dichloride, chloroform, ethylene dichloride, trieline, tetrahydrofuran (THF), second eyeball, propylene glycol, ethylene glycol, ethylene glycol monomethyl ether, glycol dimethyl ether, 1 with solvent during solvent wash, the mixture of one or more in the 4-dioxane, wash temperature is normal temperature or at 50 ℃～120 ℃, obtains the silica flour wet feed through mechanical separation again after cleaning.
- According to claim 1 a kind of from crystalline silicon cutting waste mortar resource utilization reclaim the method for silicon carbide component, its characteristic is: in step (4) described when oven dry silica flour wet feed furnace drying method used comprise fluid-bed drying, fixed bed drying method; 60 ℃～130 ℃ of bake out temperatures; Oven dry pressure comprises normal pressure or vacuum.
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| CN103496831B (en) * | 2013-09-18 | 2015-04-29 | 河南新大新材料股份有限公司 | Recycling method of silicon wafer cutting edge material waste water treatment sludge |
| CN103965791A (en) * | 2014-05-07 | 2014-08-06 | 连云港健发磁性材料有限公司 | Clean rapid regeneration method of waste rare-earth polishing powder |
| CN105948056B (en) * | 2016-05-16 | 2017-09-22 | 安徽赛华新能源科技有限公司 | Crystalline silicon cutting waste mortar online recycling utilizes production technology |
| CN108046269A (en) * | 2018-01-16 | 2018-05-18 | 常州大学 | A kind of technique of the useless powder separation and recovery of solar silicon wafers cutting |
| CN109037665B (en) * | 2018-07-10 | 2019-10-15 | 郑州中科新兴产业技术研究院 | A method of nano-silicon negative electrode material is prepared using photovoltaic industry waste silicon residue |
| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
| CN116177552B (en) * | 2023-02-22 | 2023-11-17 | 江苏秉盛环保工程有限公司 | Silicon wafer cutting fluid silicon powder recovery system and process thereof |
| CN117304997A (en) * | 2023-09-28 | 2023-12-29 | 宁夏中欣晶圆半导体科技有限公司 | Method for preparing solid fuel by utilizing silicon wafer mortar line slice waste and solid fuel |
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| JP5466455B2 (en) * | 2009-08-13 | 2014-04-09 | 信越化学工業株式会社 | Method for producing silicon carbide |
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